CN104311090B - A kind of hot pressed sintering/presoma cracking process prepares the method for Cf/ZrC-SiC ultrahigh temperature ceramic composite - Google Patents
A kind of hot pressed sintering/presoma cracking process prepares the method for Cf/ZrC-SiC ultrahigh temperature ceramic composite Download PDFInfo
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Abstract
The present invention relates to the method that a kind of hot pressed sintering/presoma cracking process prepares Cf/ZrC-SiC ultrahigh temperature ceramic composite, be specially and utilize presoma cracking process to prepare the method for Cf/ZrC-SiC ultrahigh temperature ceramic composite in conjunction with hot pressing sintering method original position.The method is by ZrSi
2powder is incorporated into carbon fibre fabric inside, by hot pressing sintering method in-situ preparation ZrC, SiC ceramic matrix, adopts presoma cracking process to carry out final densification, obtains fine and close Cf/ZrC-SiC ultrahigh temperature ceramic composite.Ultrahigh temperature ceramic composite prepared by the method has excellent applied at elevated temperature performance, and the method technological process is simple, consuming time short.The Cf/ZrC-SiC ultrahigh temperature ceramic composite obtained can meet the practical application of some thermal protection struc ture parts substantially; Reenter at hypersonic flight, atmospheric layer, have a wide range of applications in the extreme environment such as Trans-atmospheric flight and rocket propulsion system.
Description
Technical field
The present invention relates to the method that a kind of hot pressed sintering/presoma cracking process prepares Cf/ZrC-SiC ultrahigh temperature ceramic composite, be specially and utilize presoma cracking process to prepare the method for Cf/ZrC-SiC ultrahigh temperature ceramic composite in conjunction with hot pressing sintering method original position.
Background technology
Carbon fibre reinforced ceramics based composites is that a class is high temperature resistant, the thermal structure material of low density, high-strong toughness, combine the superior mechanical property of fibre reinforcement and the good chemistry of ceramic matrix and thermostability, there is density low, corrosion-resistant, mechanics, heat physical properties are excellent, Burning corrosion resistance and dynamic and static friction and wear behavior advantages of higher, can be prepared into complex-shaped engineering component.At present, chemical vapor infiltration and polymer infiltration and pyrolysis method is mainly contained for the preparation of the method for continuous carbon fibre enhancing ceramic matric composite both at home and abroad.
The technological principle of chemical vapor infiltration is placed in by fiber preform in airtight reaction chamber, and by reactant gases, at high temperature, gas infiltrates precast body inside and chemical reaction occurs, and generates ceramic matrix.Its principal feature has: the preparation 1. carrying out matrix under low-pressure low-temperature, and the internal residual stress of material is little, and fibre damage is little; 2. complex-shaped and that fiber volume fraction is high nearly size component can be prepared.But there is following shortcoming in the method: 1. matrix densification speed is low, growth cycle long (more than 100h), manufacturing cost is high; 2. be not suitable for preparing thick walled part; 3. complex process equipment, facility investment is large.
Polymer infiltration and pyrolysis method is under certain temperature and pressure; siliceous organic polymer precursor liquid solution or liquation are infiltrated up in multiporous fiber precast body; then the high-temperature heat treatment under super-dry and protection of inert gas; make presoma generation pyrolysis and obtain silicon carbide substrate, obtained carbon fibre reinforced silicon carbide composite material.Matrix composition prepared by the method is even, purity is high, and can obtain the ceramic matrix of multicomponent.But because ceramic yield in the pyrolytic process that polymkeric substance is changed to ceramic state by presoma is low, the density of material, requirement of strength be reached, often need more than ten infiltrations---pyrolysis cyclical process, preparation cycle is longer.In addition the cost of presoma is very high, causes the cost of material very high.
Therefore, for meeting the wide application demand of Ceramic Matrix Composites Reinforced by Carbon Fibers at high-temperature hot structured material, simple in the urgent need to researching and developing out production technique, cycle is short, and densifying method with low cost, the low cost realizing fibre reinforced ultra-temperature ceramic-based composite material by this method is prepared fast.The method of hot pressed sintering is incorporated in matrix material preparation process by the present invention, in preparation process, by method in-situ preparation ZrC, SiC of hot pressed sintering, polymer infiltration and pyrolysis method is adopted to be incorporated in material by SiC matrix, filling pore, reach ideal density, obtain the matrix material of excellent performance.
Summary of the invention
The object of the invention is the method preparing Cf/ZrC-SiC ultrahigh temperature ceramic composite in order to propose a kind of hot pressed sintering/presoma cracking process, ultrahigh temperature ceramic composite prepared by the method has excellent applied at elevated temperature performance, and the method technological process is simple, consuming time short.
The object of the invention is to be achieved through the following technical solutions.
A kind of hot pressed sintering/presoma cracking process of the present invention prepares the method for Cf/ZrC-SiC ultrahigh temperature ceramic composite, and the method is by ZrSi
2powder is incorporated into carbon fibre fabric inside, by hot pressing sintering method in-situ preparation ZrC, SiC ceramic matrix, adopts presoma cracking process to carry out final densification, obtains fine and close Cf/ZrC-SiC ultrahigh temperature ceramic composite; The concrete steps of the method are:
1) by ZrSi
2powder mixes with dehydrated alcohol, ZrSi
2massfraction be 50%-80%, the massfraction of dehydrated alcohol is 20%-50%, obtains slurry;
2) by step 1) slurry that obtains brushes the carbon cloth surfaces cut out uniformly, and the mass ratio of carbon cloth and slurry is 1:5-10;
3) by step 2) in brush slurry carbon cloth stack, and be placed in graphite jig, then carbon cloth together puts into high temperature hot pressing sintering oven together with graphite jig, high temperature hot pressing sintering is carried out in inert atmosphere (nitrogen or argon gas) 2 ~ 3 hours, final acquisition Cf/ZrC-SiC ultra-temperature ceramic-based composite material blank under 1800 ~ 2000 DEG C and 5 ~ 30MPa pressure.
4) Polycarbosilane and Vinylstyrene are put into beaker, mixed by agitator, churning time 1 ~ 3 hour, obtains steeping fluid; The mass ratio of Polycarbosilane and Vinylstyrene is 1:0.2-1;
5) by step 4) steeping fluid that obtains is incorporated into step 3 by vacuum-impregnated method) in prepared blank; Vacuum-impregnated method is: at certain temperature (60 ~ 80 DEG C) and pressure (0.1 ~ 0.2MPa), steeping fluid is infiltrated up in blank, dipping time is 2 ~ 3 hours, to be impregnated completely after, obtain base substrate, after being taken out by base substrate, put into solidification tank (60 ~ 80 DEG C); At certain temperature (180 ~ 200 DEG C) and pressure (0.3 ~ 3MPa), carry out cure under pressure, set time is 4 ~ 8 hours, with stove slow cooling to steeping fluid completion of cure;
6) Pintsch process: by step 5) solidification after base substrate put into high-temperature cracking furnace, at 1300 ~ 1600 DEG C, carry out Pintsch process 3 ~ 6 hours in inert atmosphere (nitrogen or argon gas), complete the pyrolytic conversion of SiC organic polymer precursor body to SiC crystal;
7) repeat above-mentioned 5), 6) step 2 ~ 3 round, final obtain fine and close Cf/ZrC-SiC ultra-temperature ceramic-based composite material.
Described ZrSi
2powder average particle size is 10 ~ 20 microns, its purity>=99%;
Described Polycarbosilane (PCS) molecular weight is 1000-1500, and Vinylstyrene (DVB) purity is 99.9%.
Beneficial effect
The object of the invention is the method preparing Cf/ZrC-SiC ultrahigh temperature ceramic composite in order to propose a kind of hot pressed sintering/presoma cracking process, ultrahigh temperature ceramic composite prepared by the method has excellent applied at elevated temperature performance, and the method technological process is simple, consuming time short.The Cf/ZrC-SiC ultrahigh temperature ceramic composite obtained can meet the practical application of some thermal protection struc ture parts substantially; Reenter at hypersonic flight, atmospheric layer, have a wide range of applications in the extreme environment such as Trans-atmospheric flight and rocket propulsion system.
Accompanying drawing explanation
The Cf/ZrC-SiC material surface XRD figure spectrum of Fig. 1 prepared by embodiment 1;
The Cf/ZrC-SiC material surface pattern back scattering photo of Fig. 2 prepared by embodiment 1;
The Cf/ZrC-SiC Fracture Profile in Metallic Materials pattern back scattering photo of Fig. 3 prepared by embodiment 1.
Embodiment
Illustrate substantive distinguishing features of the present invention and marked improvement further below by specific embodiment, but content of the present invention is not only confined to the following examples:
Embodiment 1
A kind of Cf/ZrC-SiC ultrahigh temperature ceramic composite preparation method, by ZrSi
2powder is incorporated into carbon fibre fabric inside, by hot pressing sintering method in-situ preparation ZrC, SiC ceramic matrix, adopts presoma cracking process to carry out final densification, obtains fine and close Cf/ZrC-SiC ultrahigh temperature ceramic composite.
The concrete steps of the method are:
1) by ZrSi
2powder is mixed in dehydrated alcohol, ZrSi
2massfraction be 100g, the massfraction of dehydrated alcohol is 100g, obtains slurry;
2) by step 1) slurry that obtains brushes the carbon cloth surfaces cut out uniformly, and the quality of carbon cloth and slurry is respectively 40g and 200g;
3) by step 2) in brush slurry carbon cloth stack, and be placed in graphite jig, then carbon cloth together puts into high temperature hot pressing sintering oven together with graphite jig, under 2000 DEG C and 30MPa pressure, carry out high temperature hot pressing in inert atmosphere (argon gas) sinter 3 hours, final acquisition Cf/ZrC-SiC ultra-temperature ceramic-based composite material blank;
4) Polycarbosilane and Vinylstyrene are put into beaker, mixed by agitator, churning time 3 hours, obtains steeping fluid; The quality of Polycarbosilane and Vinylstyrene is respectively 300g and 300g;
5) by step 4) steeping fluid prepared is incorporated into step 3 by vacuum-impregnated method) in prepared blank; Under 60 DEG C and 0.2MPa pressure, be infiltrated up to by steeping fluid in blank, dipping time is 2 hours, to be impregnated completely after, put into solidification tank (60 DEG C) after being taken out by base substrate; At the temperature of 200 DEG C and 3MPa pressure, carry out cure under pressure, set time is 8 hours, with stove slow cooling to presoma completion of cure.
6) Pintsch process: by step 5) solidification after base substrate put into high-temperature cracking furnace, at 1300 DEG C, carry out Pintsch process 3 hours in inert atmosphere (nitrogen or argon gas), complete the pyrolytic conversion of SiC organic polymer precursor body to SiC crystal;
7) repeat above-mentioned 4), 5), 6) step 3 round, final obtain fine and close Cf/ZrC-SiC ultra-temperature ceramic-based composite material.
The Cf/ZrC-SiC ultra-temperature ceramic-based composite material scanning electron microscope prepared by aforesaid method is observed material surface microtexture, can find out that material surface does not have obvious hole, and material density is good, as shown in Figure 2;
The Cf/ZrC-SiC ultra-temperature ceramic-based composite material scanning electron microscope prepared by aforesaid method is observed Fracture Profile in Metallic Materials pattern, can find out that fiber is intact, as shown in Figure 3;
Carry out density measurement to Cf/ZrC-SiC ultra-temperature ceramic-based composite material drainage prepared by aforesaid method, known material compactness is good, and density is 2.21g/cm
3;
The Cf/ZrC-SiC ultra-temperature ceramic-based composite material XRD diffractometer prepared by aforesaid method carries out material phase analysis, can find out that material is primarily of ZrC, SiC composition, exists without other dephasigns, as shown in Figure 1;
Carry out room temperature flexural strength test to Cf/ZrC-SiC ultra-temperature ceramic-based composite material prepared by aforesaid method by 3 curved methods, known material room temperature strength is 107MPa.
Embodiment 2
A kind of Cf/ZrC-SiC ultrahigh temperature ceramic composite preparation method, by ZrSi
2powder is incorporated into carbon fibre fabric inside, by hot pressing sintering method in-situ preparation ZrC, SiC ceramic matrix, adopts presoma cracking process to carry out final densification, obtains fine and close Cf/ZrC-SiC ultrahigh temperature ceramic composite.
The concrete steps of the method are:
1) ZrSi2 powder is mixed in dehydrated alcohol, ZrSi
2massfraction be 60%, the massfraction of dehydrated alcohol is 40%, obtains slurry;
2) by step 1) slurry that obtains brushes the carbon cloth surfaces cut out uniformly, and the mass ratio of carbon cloth and slurry is 1:8;
3) by step 2) in brush slurry carbon cloth stack, and be placed in graphite jig, then carbon cloth together puts into high temperature hot pressing sintering oven together with graphite jig, under 1900 DEG C and 30MPa pressure, carry out high temperature hot pressing in inert atmosphere (argon gas) sinter 3 hours, final acquisition Cf/ZrC-SiC ultra-temperature ceramic-based composite material blank;
4) Polycarbosilane and Vinylstyrene are put into beaker, mixed by agitator, churning time 3 hours, obtains steeping fluid; The mass ratio of Polycarbosilane and Vinylstyrene is 1:1;
5) by step 4) steeping fluid prepared is incorporated into step 3 by vacuum-impregnated method) in prepared blank.Under 60 DEG C and 0.2MPa pressure, be infiltrated up to by steeping fluid in blank, dipping time is 2 hours, to be impregnated completely after, put into solidification tank (60 DEG C) after being taken out by base substrate; At the temperature of 200 DEG C and 3MPa pressure, carry out cure under pressure, set time is 8 hours, with stove slow cooling to presoma completion of cure.
6) Pintsch process: by step 5) solidification after base substrate put into high-temperature cracking furnace, at 1500 DEG C, carry out Pintsch process 3 hours in inert atmosphere (nitrogen or argon gas), complete the pyrolytic conversion of SiC organic polymer precursor body to SiC crystal.
7) repeat above-mentioned 5), 6) step 3 round, final obtain fine and close Cf/ZrC-SiC ultra-temperature ceramic-based composite material.
The Cf/ZrC-SiC ultra-temperature ceramic-based composite material scanning electron microscope prepared by aforesaid method is observed material surface microtexture, and can find out that material surface does not have obvious hole, material density is good.
Carry out density measurement to Cf/ZrC-SiC ultra-temperature ceramic-based composite material drainage prepared by aforesaid method, known material compactness is good, and density is 2.32g/cm
3;
The Cf/ZrC-SiC ultra-temperature ceramic-based composite material XRD diffractometer prepared by aforesaid method carries out material phase analysis, can find out that material is primarily of ZrC, SiC composition, exists without other dephasigns.
Carry out room temperature flexural strength test to Cf/ZrC-SiC ultra-temperature ceramic-based composite material prepared by aforesaid method by 3 curved methods, known material room temperature strength is 116MPa.
Embodiment 3
A kind of Cf/ZrC-SiC ultrahigh temperature ceramic composite preparation method, by ZrSi
2powder is incorporated into carbon fibre fabric inside, by hot pressing sintering method in-situ preparation ZrC, SiC ceramic matrix, adopts presoma cracking process to carry out final densification, obtains fine and close Cf/ZrC-SiC ultrahigh temperature ceramic composite.
The concrete steps of the method are:
1) by ZrSi
2powder is mixed in dehydrated alcohol, ZrSi
2massfraction be 80%, the massfraction of dehydrated alcohol is 20%, obtains slurry;
2) by step 1) slurry that obtains brushes the carbon cloth surfaces cut out uniformly, and the mass ratio of carbon cloth and slurry is 1:10;
3) by step 2) in brush slurry carbon cloth stack, and be placed in graphite jig, then carbon cloth together puts into high temperature hot pressing sintering oven together with graphite jig, under 1800 DEG C and 10MPa pressure, carry out high temperature hot pressing in inert atmosphere (argon gas) sinter 3 hours, final acquisition Cf/ZrC-SiC ultra-temperature ceramic-based composite material blank.
4) Polycarbosilane and Vinylstyrene are put into beaker, mixed by agitator to two kinds of solvents, churning time 3 hours, obtains steeping fluid; The mass ratio of Polycarbosilane and Vinylstyrene is 1:1;
5) by step 4) steeping fluid prepared is incorporated into step 3 by vacuum-impregnated method) in prepared blank.Under 80 DEG C and 0.1MPa pressure, be infiltrated up to by steeping fluid in blank, dipping time is 2 hours, to be impregnated completely after, put into solidification tank (80 DEG C) after being taken out by base substrate; At the temperature of 180 DEG C and 1MPa pressure, carry out cure under pressure, set time is 8 hours, with stove slow cooling to presoma completion of cure.
6) Pintsch process: by step 5) solidification after base substrate put into high-temperature cracking furnace, at 1600 DEG C, carry out Pintsch process 3 hours in inert atmosphere (nitrogen or argon gas), complete the pyrolytic conversion of SiC organic polymer precursor body to SiC crystal.
7) repeat above-mentioned 5), 6) step 3 round, final obtain fine and close Cf/ZrC-SiC ultra-temperature ceramic-based composite material.
The Cf/ZrC-SiC ultra-temperature ceramic-based composite material scanning electron microscope prepared by aforesaid method carries out microstructure observation, and can find out that material surface does not have obvious hole, material density is good.
Carry out density measurement to Cf/ZrC-SiC ultra-temperature ceramic-based composite material drainage prepared by aforesaid method, known material compactness is good, and density is 2.27g/cm
3;
The Cf/ZrC-SiC ultra-temperature ceramic-based composite material XRD diffractometer prepared by aforesaid method carries out material phase analysis, can find out that material is primarily of ZrC, SiC composition, exists without other dephasigns.
Carry out room temperature flexural strength test to Cf/ZrC-SiC ultra-temperature ceramic-based composite material prepared by aforesaid method by 3 curved methods, known material room temperature strength is 109MPa.
Claims (4)
1. hot pressed sintering/presoma cracking process prepares a method for Cf/ZrC-SiC ultrahigh temperature ceramic composite, it is characterized in that:
The concrete steps of the method are:
1) by ZrSi
2powder mixes with dehydrated alcohol, ZrSi
2massfraction be 50%-80%, the massfraction of dehydrated alcohol is 20%-50%, obtains slurry;
2) by step 1) slurry that obtains brushes the carbon cloth surfaces cut out uniformly, and the mass ratio of carbon cloth and slurry is 1:5-10;
3) by step 2) in brush slurry carbon cloth stack, and be placed in graphite jig, then carbon cloth together puts into high temperature hot pressing sintering oven together with graphite jig, under 1800 ~ 2000 DEG C and 5 ~ 30MPa pressure, in inert atmosphere, carry out high temperature hot pressing sintering 2 ~ 3 hours, obtain Cf/ZrC-SiC ultrahigh temperature ceramic composite blank;
4) Polycarbosilane and Vinylstyrene are put into beaker, mixing, obtains steeping fluid; The mass ratio of Polycarbosilane and Vinylstyrene is 1:0.2-1;
5) by step 4) steeping fluid that obtains is incorporated into step 3 by vacuum-impregnated method) in prepared blank; Vacuum-impregnated method is: at the temperature of 60 ~ 80 DEG C and 0.1 ~ 0.2MPa pressure, be infiltrated up to by steeping fluid in blank, and dipping time is 2 ~ 3 hours, to be impregnated completely after, obtain base substrate, will base substrate take out after put into the solidification tank of 60 ~ 80 DEG C; At 180 ~ 200 DEG C of temperature and 0.3 ~ 3MPa pressure, carry out cure under pressure, set time is 4 ~ 8 hours, with stove slow cooling to steeping fluid completion of cure;
6) by step 5) solidification after base substrate put into high-temperature cracking furnace, Pintsch process is carried out in inert atmosphere 3 ~ 6 hours at 1300 ~ 1600 DEG C, complete the pyrolytic conversion of SiC organic polymer precursor body to SiC crystal, obtain Cf/ZrC-SiC ultrahigh temperature ceramic composite.
2. a kind of hot pressed sintering/presoma cracking process according to claim 1 prepares the method for Cf/ZrC-SiC ultrahigh temperature ceramic composite, it is characterized in that: the method also comprises step 7): repeat above-mentioned 5), 6) step 2-3 round, final obtain fine and close Cf/ZrC-SiC ultrahigh temperature ceramic composite.
3. a kind of hot pressed sintering/presoma cracking process according to claim 1 prepares the method for Cf/ZrC-SiC ultrahigh temperature ceramic composite, it is characterized in that: ZrSi
2powder average particle size is 10 ~ 20 microns, its purity>=99%.
4. a kind of hot pressed sintering/presoma cracking process according to claim 1 prepares the method for Cf/ZrC-SiC ultrahigh temperature ceramic composite, it is characterized in that: Polycarbosilane molecular weight is 1000-1500, and Vinylstyrene purity is 99.9%.
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